May J C, Wheeler R M, Grim E
Department of Health and Human Services, Food and Drug Administration, Bethesda, Maryland 20892.
Cryobiology. 1989 Jun;26(3):277-84. doi: 10.1016/0011-2240(89)90023-0.
The gravimetric test for the determination of residual moisture in freeze-dried biological products performed in a humidity- and temperature-controlled room with the use of scrupulous gravimetric analytical technique can be used to accurately determine residual moisture in freeze-dried biological products such as antihemophilic factor (human) or honey bee venom allergenic extract. This method determines the first water of hydration of sodium tartrate dihydrate (7.93%) to within 1.3% of the calculated value with a relative standard deviation of 0.3% for 10 replicates. For this gravimetric procedure, freeze-dried samples containing from 1.12 to 4.4% residual moisture had relative standard deviations ranging from 3.6 to 9.1%. Samples containing less than 1.0% residual moisture by the gravimetric method such as intravenous immune globulin and antihemophilic factor (human) had relative standard deviations ranging from 16.7 to 47.0%. Relative standard deviations for residual moisture tests performed on comparable samples by the Karl Fischer and thermogravimetric methods showed similar variability.
在湿度和温度可控的房间内，采用严谨的重量分析技术对冻干生物制品中的残留水分进行重量测定试验，可用于准确测定冻干生物制品（如抗血友病因子（人）或蜜蜂毒液变应原提取物）中的残留水分。该方法测定酒石酸钠二水合物的第一水合水（7.93%），测定值与计算值的偏差在1.3%以内，10次重复测定的相对标准偏差为0.3%。对于该重量法，残留水分含量为1.12%至4.4%的冻干样品的相对标准偏差为3.6%至9.1%。通过重量法测定残留水分含量低于1.0%的样品（如静脉注射免疫球蛋白和抗血友病因子（人））的相对标准偏差为16.7%至47.0%。采用卡尔费休法和热重分析法对可比样品进行残留水分测试的相对标准偏差显示出类似的变异性。
